EP1286916A1 - Production of activated carbon exhibiting an elevated catalytic activity - Google Patents
Production of activated carbon exhibiting an elevated catalytic activityInfo
- Publication number
- EP1286916A1 EP1286916A1 EP01949235A EP01949235A EP1286916A1 EP 1286916 A1 EP1286916 A1 EP 1286916A1 EP 01949235 A EP01949235 A EP 01949235A EP 01949235 A EP01949235 A EP 01949235A EP 1286916 A1 EP1286916 A1 EP 1286916A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- activated carbon
- carbon substrate
- activation
- volume
- gas mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8603—Removing sulfur compounds
- B01D53/8609—Sulfur oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/336—Preparation characterised by gaseous activating agents
Definitions
- the present invention relates to a process for producing activated carbon with increased catalytic activity, the process starting from an activated carbon substrate.
- the process of the invention is based on an activated carbon substrate based on carbon-containing coking materials.
- Activated carbon with increased catalytic activity has been of particular interest in various areas for some time.
- Activated carbon with an increased activity for SO 2 is of great importance for use to keep the air clean, particularly in the case of thin-film filters, since it converts and adsorbs SO 2 by adsorption-catalyzing in moist air into sulfuric acid.
- the catalytic activity can be attributed to the nitrogen content in the activated carbon, a controlled introduction of nitrogen into the activated carbon during its production being found to be advantageous over the use of nitrogen-rich starting materials.
- U.S. Pat. Nos. 5,352,370, 5,356,849, and 5,444,031 disclose processes starting from a fat or bituminous coal which is subjected to low-temperature carbonization and oxidation, followed by contacting with a small amount of a nitrogen-containing compound, e.g. Urea, during the subsequent caicination and condensation of the carbon structure.
- a nitrogen-containing compound e.g. Urea
- This caicination takes place at temperatures between 850 and 950 ° C and is carried out under an inert atmosphere.
- the nitrogen-treated high-temperature coals are then activated to a desired density at temperatures above 700 ° C. in water vapor or carbon dioxide without the addition of auxiliaries, such as air.
- the calcined and activated activated carbon is cooled to temperatures below 400 ° C. in an oxygen-free atmosphere, with cooling to below the production of the starting activated carbon is mentioned without these publications containing a more detailed description or explanation of the use of these materials.
- DE 23 52 790 C3 discloses a process for removing sulfur oxides and / or nitrogen oxides from exhaust gases, in which activated or post-treated activated carbon is used.
- This aftertreated activated carbon was made by contacting activated carbon, which according to the disclosure was produced from materials such as charcoal, coke, coconut shells, etc., with gaseous
- Ammonia generated under heat It is disclosed that the ammonia in a mixture in an inert carrier gas such as e.g. Nitrogen or flue gas is used.
- an inert carrier gas such as e.g. Nitrogen or flue gas is used.
- the proportion of the inert gas is in the range from 0 to about 90% by volume, based on the gaseous ammonia. The presence of other gases that are important for the activation is not disclosed.
- the object of the present invention is to enrich the state of the art at least by a further process for the production of activated carbon with increased catalytic activity, in particular a process for the production of activated carbon with increased catalytic activity for SO 2 . It is a further object of the present invention to provide a process in which as few process steps as possible for the production of activated carbon with increased catalytic activity are required, the process should lead to a defined product if possible and should be particularly economical to carry out.
- the present object is achieved according to the invention by a method according to appended claim 1.
- An alternative solution is the subject of claim 2.
- Advantageous embodiments of this method are the subject of subclaims 3 to 9.
- the method according to the invention is particularly advantageous because it basically consists of a single method step, which consists of three sub-steps which continuously merge into one another. This is already a significant simplification compared to the processes known from the prior art, in which the nitrogen enrichment in the activated carbon and the activation are carried out in two process steps which are clearly separate from one another.
- Reaction gas mixture or inert conditions is carried out.
- the activated carbon substrate to be activated is soaked with ammonia water, so that the activation takes place with the addition of CO 2 and / or H 2 O.
- a variant of the method advantageously eliminates the need for metering in gaseous ammonia and only a slight introduction of steam or water is required. As a result, the process engineering effort is considerably reduced.
- Nitrogen content in the air in the reaction gas mixture still contain N 2 .
- the heating is carried out by introducing the activated carbon substrate into a reactor preheated to the activation temperature. It goes without saying that the activated carbon substrate, as in the rest of the process, is moved sufficiently to ensure uniform contacting of the activated carbon substrate with the reactor walls and the gas phase which transmit the required heat.
- a heating rate occurs which does not require any complex regulation and special checking.
- the activation temperature is 800 to 970 ° C., since the increase in the nitrogen content and the activation of the activated carbon substrate with the reaction gas mixture according to the invention generally leads to activated carbons with particularly favorable catalytic and adsorption properties in this temperature range.
- a temperature range from 880 to 970 ° C. is preferred.
- the gas mixture used to activate the heated activated carbon substrate contains 1 to 20% by volume of NH 3 , 10 to 60% by volume of H 2 O and 5 to 50% by volume of CO 2 , 1 to 10% by volume of NH 3 , 10 to 30% by volume of H 2 O and 5 to 15% by volume of CO 2 are preferred.
- the remaining part is nitrogen.
- Activation is generally over a period of 30 to 90
- the activation is generally carried out until the desired catalytic activity for SO 2 has been reached or until the conversion to produce an activated carbon product with the desired porosity has been reached.
- the activated carbon substrate used is an activated carbon made from coconut shells.
- Activated carbon based on coconut shells is particularly suitable for the production of activated carbon with increased catalytic activity, since it already has an extremely favorable pore structure, which surprisingly is particularly beneficial for increasing the nitrogen content and thus affects the catalytic activity and the adsorptive properties of the process product.
- this starting material can be obtained commercially in a constant quality, in sufficient quantity and inexpensively.
- the activated activated carbon substrate is cooled to a temperature of ⁇ 200 ° C. This ensures in the reaction gas atmosphere that an unwanted change in the activated carbon substrate does not occur due to atmospheric oxygen.
- the activated carbon substrate at a temperature ⁇ 200 ° C can also be easily discharged from the reactor used and sent to intermediate storage or further processing without special precautions regarding the temperature resistance of the devices and containers coming into contact with the process product.
- the tube was then inserted horizontally into a tube furnace heated to the activation temperature, the temperature being kept constant during the heating of the activated carbon in the tube.
- the tube was rotated at a speed of about 6 revolutions / minute.
- the gas used to increase the catalytic activity and for activation was passed through the tube and over the activated carbon, the tube being removed from the tube furnace together with the activated carbon after 60 minutes.
- the process product was then cooled to a temperature ⁇ 200 ° C. under an N 2 atmosphere. Finally, the tube was emptied and the activated carbon thus obtained and treated was subjected to an appropriate analysis.
- the analytical data of the starting material used as an activated carbon substrate based on coconut shells are as follows:
- An activated carbon substrate was treated in accordance with the above information.
- a combination of NH 3 , CO 2 and H 2 O is used as the gas mixture.
- This gas mixture is obtained by heating a 25% ammonia solution while simultaneously introducing CO 2 gas.
- the activation temperature ranged from 900 to 920 ° C.
- the combustion of the carbon of the activated carbon is a maximum of 16%. Due to the change in the surface structure of the activated carbon due to the incorporation of nitrogen, the nitrogen content of the activated carbon increasing from about 0.08% to 0.3 to 0.4%, and the increased erosion, there is an increase in the specific surface area, the micropore volume and the iodine number , the reactivity and the adsorption capacity for SO 2 and for n-butane and toluene.
- the passage of the gas mixture mentioned was carried out at the following rate: 36 l / h NH 3 , 102 l / h H 2 O and 70 l / h CO 2 , which leads to a total gas volume of 208 l / h. In percentage terms, the gas mixture used was composed of 17% by volume of NH 3 , 49% by volume of H 2 O and 34% by volume of CO 2 .
- Example 2 The procedure was the same as in Example 1, except that the gas mixture was passed through at the following rate: 30 l / h NH 3> 85 l / h H 2 O and 70 l / h CO 2 , resulting in a total gas volume of 185 l / h h led.
- the gas mixture used in this example was composed of 16% by volume of NH 3 , 46% by volume of H 2 O and 38% by volume of CO 2 .
- Example 2 This example was also experienced as in Example 1, except that the gas mixture was passed through at the following rate: 24 l / h NH 3 , 68 l / h H 2 O and 70 l / h CO 2 , resulting in a total amount of gas of 162 l / h led.
- the gas mixture used in this example was composed of 15% by volume of NH 3 , 42% by volume of H 2 O and 43% by volume of CO 2 .
- the process product obtained in this way had the following properties:
- the process product thus obtained had the following properties:
- a gas mixture according to Example 1 was also used when carrying out this example, but the activation temperature was set to 880 to 900 ° C.
- the process product obtained under these conditions had the following properties:
- Example 2 a gas mixture according to Example 1 was also used.
- the set activation temperature was 930 to 950 ° C.
- the process product obtained under these conditions had the following properties:
- Examples 7 and 8 were carried out on an industrial scale and in a continuous manner.
- activated carbon and reaction gas are conducted in cocurrent.
- the reaction gases are generated by direct combustion of
- the ammonia gas is supplied with the activated carbon, while the water vapor is also blown into the reaction chamber.
- example 7 is activated with NH 3 and H 2 O, in example 8 only with H 2 O.
- the rotary kiln is preheated with natural gas to a temperature of approx. 920 ° C and then the coal is metered in together with the ammonia gas.
- the activated carbon is transported through the furnace by rotating the pipe, which is inclined to the discharge.
- the activated carbon which has undergone the process according to the invention, is discharged via a coil and at the same time cooled to a temperature ⁇ 200 ° C.
- the process conditions were as follows:
- the gas composition according to the invention is the cause of the special properties of the activated carbon produced by the process according to the invention.
- Examples 7, 8 and 9 serve to illustrate a technical implementation of the method in a rotary kiln.
- the properties achieved here in the process products are economically sensible and usable, so that a process is available which can be used on a commercial scale without further adjustments.
- the process according to the invention already offers special advantages over processes from the prior art simply by reducing the complexity of the process - basically only one reaction step is still required.
- the process remains entirely variable and can be adapted to the respective requirements, e.g. Activity of the activated carbon or the type of starting material used can be adapted without special effort.
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10028654 | 2000-06-09 | ||
DE10028654A DE10028654A1 (en) | 2000-06-09 | 2000-06-09 | Reactivation of activated charcoal, used in thin film filter for air purification by adsorption and catalytic reaction of sulfur dioxide, involves heating to activation temperature in gas containing ammonia, carbon dioxide and/or steam |
PCT/DE2001/002087 WO2001094261A1 (en) | 2000-06-09 | 2001-06-01 | Production of activated carbon exhibiting an elevated catalytic activity |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1286916A1 true EP1286916A1 (en) | 2003-03-05 |
EP1286916B1 EP1286916B1 (en) | 2004-11-03 |
Family
ID=7645276
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP01949235A Revoked EP1286916B1 (en) | 2000-06-09 | 2001-06-01 | Production of activated carbon exhibiting an elevated catalytic activity |
Country Status (6)
Country | Link |
---|---|
US (1) | US7214645B2 (en) |
EP (1) | EP1286916B1 (en) |
AT (1) | ATE281410T1 (en) |
AU (1) | AU2001270463A1 (en) |
DE (2) | DE10028654A1 (en) |
WO (1) | WO2001094261A1 (en) |
Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20070191571A1 (en) * | 2006-02-14 | 2007-08-16 | Sink Chester W | Resol beads, methods of making them, and methods of using them |
US20070191572A1 (en) * | 2006-02-14 | 2007-08-16 | Tustin Gerald C | Resol beads, methods of making them, and methods of using them |
US20070207917A1 (en) * | 2006-02-14 | 2007-09-06 | Chester Wayne Sink | Activated carbon monoliths and methods of making them |
US8247072B2 (en) * | 2006-02-14 | 2012-08-21 | Eastman Chemical Company | Resol beads, methods of making them and methods of using them |
DE102006046880A1 (en) * | 2006-10-04 | 2008-04-10 | Carbotech Ac Gmbh | Process for the production of activated carbon with high catalytic activity |
DE102007020421A1 (en) * | 2007-04-27 | 2008-10-30 | Rwe Power Ag | Process for the preparation of elemental sulfur doped carbonaceous adsorbents and methods for exhaust gas purification using such adsorbents |
DE102008000890A1 (en) * | 2008-03-31 | 2009-10-01 | Carbotech Ac Gmbh | Activated carbon catalyst |
DK2847127T3 (en) * | 2012-05-07 | 2020-10-26 | Carbon Tech Holdings Llc | Continuous process for the production of biogenic activated carbon |
JP6512457B2 (en) * | 2013-04-05 | 2019-05-15 | エマージ リミテッド ライアビリティ カンパニー | Carbon carbide and articles formed therefrom |
CN104129777B (en) * | 2014-08-26 | 2016-03-30 | 武汉科技大学 | A kind of multifunction charcoal and preparation method thereof |
CN107159120B (en) * | 2017-06-16 | 2019-09-27 | 华中科技大学 | A kind of biology coke physical chemistry joint activation method |
WO2019047155A1 (en) * | 2017-09-08 | 2019-03-14 | 南京林业大学 | Method for preparing nitrogen-containing activated carbon by activation of ammonia gas |
JP7104273B1 (en) | 2021-10-19 | 2022-07-21 | 株式会社ファンデクセル | Coagulant and excrement treatment bag using it |
Family Cites Families (24)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE139067C (en) | ||||
DE78562C (en) | Gebr. REICHSTEIN, Brandenburg a. H | Luggage locker with two bolts moving in opposite directions | ||
JPS5111037B2 (en) | 1973-04-26 | 1976-04-08 | ||
DD139067A3 (en) * | 1974-10-25 | 1979-12-12 | Hans Hoppe | PROCESS FOR THE PREPARATION OF ACTIVATED CARBON |
JPS60167927A (en) | 1977-03-22 | 1985-08-31 | Toyobo Co Ltd | Production of nitrogen-containing active carbon fiber |
US4212852A (en) * | 1977-05-06 | 1980-07-15 | Takeda Chemical Industries, Ltd. | Method of deodorizing gas containing hydrogen sulfide and ammonia and/or amines |
JPS6052860B2 (en) | 1978-04-13 | 1985-11-21 | 武田薬品工業株式会社 | How to regenerate activated carbon |
JPS591803B2 (en) | 1978-06-30 | 1984-01-14 | 東邦ベスロン株式会社 | Method for manufacturing activated carbon fiber |
JPS5650107A (en) | 1979-09-28 | 1981-05-07 | Toho Rayon Co Ltd | Manufacture of fibrous activated carbon |
JPS57106516A (en) | 1980-12-22 | 1982-07-02 | Takeda Chem Ind Ltd | Manufacture of activated carbon |
US4624937A (en) | 1984-05-10 | 1986-11-25 | Monsanto Company | Process for removing surface oxides from activated carbon catalyst |
DE3801457A1 (en) | 1988-01-20 | 1989-08-03 | Hasso Von Bluecher | Activated carbon having high abrasion resistance and low moisture sensitivity |
US4957897A (en) | 1988-01-29 | 1990-09-18 | Rohm And Haas Company | Carbonaceous adsorbents from pyrolyzed polysulfonated polymers |
JPH0297414A (en) * | 1988-10-01 | 1990-04-10 | Kansai Coke & Chem Co Ltd | Production of active carbon having superior quality |
US6114273A (en) * | 1993-01-21 | 2000-09-05 | Calgon Carbon Corporation | Method for sox removal by catalytic carbon |
US5356849A (en) * | 1993-01-21 | 1994-10-18 | Calgon Carbon Corporation | Catalytic carbon |
US5700436A (en) * | 1993-01-21 | 1997-12-23 | Calgon Carbon Corporation | Purification of air in enclosed spaces |
US5444031A (en) * | 1993-01-21 | 1995-08-22 | Calgon Carbon Corporation | Process for making catalytic carbon |
US5352370A (en) | 1993-01-21 | 1994-10-04 | Calgon Carbon Corporation | Method for SOx removal by catalytic carbon |
CA2134160C (en) * | 1993-10-25 | 1999-12-14 | Frederick S. Baker | Highly microporous carbons and process of manufacture |
US5959126A (en) | 1997-10-29 | 1999-09-28 | Flexsys America L. P. | Formation of quinonedimines from phenylenediamines by catalytic oxidation |
US6187937B1 (en) | 1998-01-16 | 2001-02-13 | Flexsys America L.P. | Preparation of N-phenyl-benzoquinoneimine from hydroxydiphenylamines |
US6342129B1 (en) | 1998-05-14 | 2002-01-29 | Calgon Carbon Corporation | Process for production of carbonaceous chars having catalytic activity |
CN1068913C (en) * | 1998-10-07 | 2001-07-25 | 中国科学院山西煤炭化学研究所 | Preparation of active carbon fiber with high desulfurization rate |
-
2000
- 2000-06-09 DE DE10028654A patent/DE10028654A1/en not_active Ceased
-
2001
- 2001-06-01 US US10/297,547 patent/US7214645B2/en not_active Expired - Lifetime
- 2001-06-01 WO PCT/DE2001/002087 patent/WO2001094261A1/en active IP Right Grant
- 2001-06-01 EP EP01949235A patent/EP1286916B1/en not_active Revoked
- 2001-06-01 AU AU2001270463A patent/AU2001270463A1/en not_active Abandoned
- 2001-06-01 AT AT01949235T patent/ATE281410T1/en not_active IP Right Cessation
- 2001-06-01 DE DE50104403T patent/DE50104403D1/en not_active Expired - Lifetime
Non-Patent Citations (1)
Title |
---|
See references of WO0194261A1 * |
Also Published As
Publication number | Publication date |
---|---|
ATE281410T1 (en) | 2004-11-15 |
DE10028654A1 (en) | 2001-12-20 |
AU2001270463A1 (en) | 2001-12-17 |
DE50104403D1 (en) | 2004-12-09 |
US7214645B2 (en) | 2007-05-08 |
WO2001094261A1 (en) | 2001-12-13 |
US20030153458A1 (en) | 2003-08-14 |
EP1286916B1 (en) | 2004-11-03 |
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